Back Titration

Qualitative Analysis: -1 It determines the presence or absence of a particular

compound, but not the mass or concentration.

By definition , qualitative analysis do not measure

quantity.

Quantitative Analysis: -2 It determines how much of each component , or of

specified components is present in a given sample.

Methods of Quantitative Chemical Analysis : 1-Volumetric ( Titrimetric ) analysis.

2-Gravimetric analysis.

3-Spectrophotometric analysis.

The reaction can be represented

by a chemical equation.

The reaction should be relatively fast.

The reaction should be complete & irreversible.

The end point should be easily detected.

Requirements For a Titremetric

Assay:

Types of Titration: 1- Forward titration (direct titration).

2- Back titration (indirect titration).

Back Titration:

It includes the addition of an excess of a std. solution

to a weighted amount of a sample and then the excess

unreacted std. solution is determined by titration with

another std. solution.

Back Titration Is Used For:

1- Volatile substances, e.g., NH3 .

2- Insoluble or slightly soluble substances, e.g. CaCO3

3- Substances for which the quantitative reaction

proceeds rapidly only in the presence of excess

of reagent, e.g., Lactic acid & Aspirin.

4- Substances which decompose on heating, e.g. ,

Formaldehyde.

Principle: The determination of the amount of aspirin present in a tablet dosage form is done by alkaline hydrolysis of aspirin using N/2 NaOH standard solution followed by back titrating of the excess unreacted alkali using N/2 HCl std. solution & phenol red as indicator.

Titration of the excess

unreacted alkali with

N/2 HCl std. solution

using phenol red

indicator

Aspirin readily dissolved in dilute

NaOH solution and hydrolyzed

completely by heating for 10 minutes

with an excess of a base.

As in other quantitative determination

involving boiling with a standard alkali ,

cooling and back titrating the excess, it’s

necessary to carry out

a blank experiment

without the aspirin

In order to: 1- Minimize any error due

to small unavoidable

losses.

2- Heating and cooling an

alkaline liquid results

in an apparent change

in strength if certain

indicators are used .

A separate

determination

, the sample

being omitted,

under exactly

the same

experimental

conditions as

employed in

the actual

analysis of the

sample.

COOH

OC

O

CH3

+ 2 NaOH

COO- Na

+

OH

+ CH3COONa

Aspirin N/2 Sod. hydroxide Sod. salicylate Sod. acetate

This change may be due to the interaction of

the reagent with the glass or due to , the

absorption of atmospheric CO2 ,

CO2 is rapidly absorbed by the hot alkaline

solution to form sodium carbonate .

In the back titration with the standard acid

the librated CO2 causes a color change of the

indicator before the actual end point.

2 NaOH + CO2 Na2CO3 + H2O

Na2CO3 + 2 HCl 2 NaCl + CO2 + H2O

CO2 + H2O H2CO3 False end point

Phenol Red Indicator:

It’s also known as phenolsulfonphthalein

. pH indicator( PSP ) is a

http://en.wikipedia.org/wiki/File:Phenol-red-zwitterionic-form-2D-skeletal.pnghttp://en.wikipedia.org/wiki/PH_indicator

Chemical

Factor

A student had crushed 20 aspirin

tablets ( 0.3 g aspirin each ) ,

recorded the weight of the powder

as 6.5 g & he quantitatively

analyzed aspirin by back titration .

Using 0.5 g of crushed powdered sample, N/2 NaOH

& N/2 HCl std. sln. He recorded the results in the

following data table:

Blank exp. Sample exp.

_____ 0.5 g Weight of the powdered aspirin used

30 ml 30 ml Volume of 0.49 N NaOH used

28 ml 19 ml Volume of 0.51 N HCL consumed

Each 0.045 g of aspirin 1 ml of 0.5 N NaOH std. sln.

1 ml of 0.5 N HCl std. sln.

1- Calculate the average weight of an individual

aspirin tablet? Answer:

The average wt. of an individual tablet = 6.5 / 20

= 0.325 g

2- How many grams of aspirin ( pure ) is present in

the student's sample? Answer:

1st We should correct the normality of the used HCl to

0.5 N

2nd We should also correct the volume of blank

3rd Calculate the volume of 0.5 N HCl reacted with

pure aspirin indirectly.

4th Calculate the amount of pure aspirin present in the

sample by using the calculated Chemical Factor.

Each 1ml of 0.5 N HCl is equivalent to 0.045 g of Aspirin.

1- Why did you use your burette and not

a graduated cylinder to add the excess

NaOH standard solution?

2- What is the definition of:

a- Titration?

b- Equivalence point?

c- End point?

d- Standard solution?

e- Indicator?

f- Molarity & Normality?